Apparatus for drying hexachlorethane



Dec. 13, 19321 R MYERS 1,890,654

APPARATUS FOR DRYING HEXACHLORETHANE Filed June-25, 1929 2 Sheets-Sheet 1 l; X ufi INVENTOR. Holland D Myers Y A TTORNEYJ.

Dec. 13, 1932. MYERs 1,890,654

APPARATUS FOR DRYING HEXACHLORETHANE Filed June 25, 1929 2 Sheets-Sheet 2 Fig. 3

INVENTOR. Holland fllfyem BY A TTORNEYS.

Patented Dec. 13, 1932 UNITED STATES HOLLAND D. MYERS, F EDGEWOOD ARSENAL, MARYLAND APPARATUS FOR DRYING HEXACHLORETHANE Application filed June 25, 1929. Serial No. 373,674.

(GRANTED UNDER THE ACT OF MARCH 3, 1883, AS AMENDED APRIL 30, 1928; 370 O. G. 757) This invention described herein may be manufactured and used by or for the Government for government purposes, without the payment to me of any royalty thereon.

This invention relates in general to removing contained liquids from volatile solids having a low inter'solubility therewithin the liquid phase, and more particularly has reference to a process and apparatus for drying o hexachlorethane.

Previous to this time, the various methods employed for removing contained liquids from materials of this character have not usually proved well suited for practical purposes. In the past, it has been customary in drying solids, of thetype of hexachlorethane for example, to centrifuge the wet material to reduce the mo sture content to as low a degree as practical.

The remaining traces of water have been removed to the greatest possible extent by bringing the material in contact with relatively dry air. In carrying on an air-drying operation of this type, however, a large percentage of the solid under treatment is lost,

ranging in many instances from an approximate of around ten to over fifteen per cent.

An object of this invention is to provide a process and apparatus for removing contained liquids from volatile solids having a low intersolubility therewith in the liquid phase without any appreciable loss of the normally solid material.

Another object of this invention is to provide a process and apparatus for removing contained liquids from volatile solids having a low intersolubility therewith in the liquid phase without any appreciable loss of the normally solid material in which the contained liquid is separated and removed.

Still another object of this invention is to provide a process and apparatus for removing contained liquids from volatile solids 5 having a low intersolubility therewith in the liquid phase without any appreciable'loss of the normally solid material in which the solid is separated in the liquid phase and removed.

59 A further object of this invention is to provide a process of drying hexachlorethane without any appreciable loss of the material.

This invention contemplates in general removing contained liquids from volatile solids having a low intersolubility therewith in the liquid phase by liquefying the solid in a closed vessel and efiecting a separation of the liquid layers so as to obtain a product substantially free from moisture.

With these and other objects in View which 60 may be incident to my improvements, the invention consists in the parts and combinations to be hereinafter set forth and claimed, with the understanding that the several necessary elements comprising my invention may be varied in construction, proportions and arrangement, without departing, from the spirit and scope of the appended claims.

In order to make my invention more clearly understood, I have shown in the accom- 7 panying drawings means for carrying the same into practical efiect, without limiting the improvements in their useful applications to the particular constructions which for the purpose of explanation have been made the subject of illustration.

In the drawings forming a part of this specification i Figure 1 is a side elevational view, partly in section, of one form of apparatus suitable s0 for carrying on the process forming the subject matter of this invention, in which the contained liquid may be drawnofi? and the solid material removed in a body.

Figure 2 is a sectional view taken on line A-A of Figure 1. I

Figure 3 is a sectional view of another form of apparatus in which the contained liquid may be decanted and the normally solid material drawn oif in the liquid phase. Referring'by numerals to the drawings, and more particularly to Figure 1, there is shown an apparatus suitable for carrying on the process which will be described with reference to one specific application of the invention consisting in the drying of hexachlorethane. The apparatus comprises a pressure resistant container or autoclave 1 having a flanged rim 2 on which is fitted a dome closure or cover 3 formed with a corresponding flange 4.

The flanges 2 and 4 are preferably held together to make a tight joint by a plurality of nuts and bolts 5 and 6, although it is evident that any other convenient form of mounting may be employed if so desired.

A plurality of trunnions are provided on the opposite sides of the autoclave either formed thereon or otherwise attached, adapted to rotate in bearings 7 formed on a frame 8. This type of mounting allows for rotation of the autoclave for a purpose to be more fully hereinafter understood. A pinion wheel 9 is fixedly mounted on one of the trun- HiOES 6 adapted to be engaged by a pinion 11 fixed to a shaft 12 extending through a proj ection formed on the frame 8 and operated through a crank 13. It will thus be seen that by rotation of the crank, the autoclave may be rotated on the trunnions to any desired degree. c

The closure 3 is formed with a tubular recess or well with walls 14 having an inwardly extending flange 15 at the bottom of" which there is adapted to be seated a sight glass 16. The glass is fixed on the flange 15 by a disk 17 bolted thereto as at 18, and a leakproof joint insured by washers, or otherwise fixed'in the well in any other practical manner.

A conduit 19 is formed in the cover directly below the well having a skimmer 21 provided on the bottom edge thereof, extending 'to a point in line with the center of the sight glass. The end of an outlet line 22 is fixed in the conduit, having a valve 23 interposed therein to control the flow of the contents of the autoclave.

' A thermometer 24 is mounted in the wall of the autoclave in the conventional manner and the usual pressure gauge 25 and pressure control valve 26 provided on the top of the closure. The center of the closure is provided in addition with a ring 27, made integral therewith or suitably attached, to allow purchase for a tool to aid in removing and re l 1' piaung the cover.

A burner 28 is positioned below the bottom of the autoclave to heat the contents, and

tinctly understood that in carrying out the process, the invention is in nowise restricted to the part1cular apparatus described, as will be later understood. In the same manner, the

. may be recovered.

apparatus may be used for treating any other materials besides hexachlorethane, such for example as the drying of napthalene, borneol, anthracene or any other volatile solid having a low intersolubilit-y with a contained liquid at or above the melting point of the solid.

In drying hexachlorethane, the cover of the autoclave, which is positioned upright, is first opened and a charge of the material introduced, preferably to the level of the flange 2, whereupon the closure is replaced and made secure, a leakproof joint between the flanges being insured. The autoclave is then heated through the agency of the burner 28 until the hexachlorethane within is melted, liquefaction taking placeat around 184 (1, which temperature may be noted on the thermometer 2e, and a pressure of approximately 160 pounds 1 er square inch generated, which may be observed from the gauge 25. An excessive rise in temperature or pressure may be controlled by regulation of the gas supplied to the burner and opening of the valve 26. it has been found that both the temperature tain limits according to the amount of impurities present. I

The molten hexachlorethane has a specific gravity of approximately 2.0, or twice that of water, so that it separates from the water" in a distinct layer. The interface between the layers is usually plainly discernible, although it may be found advisable in some instances to provide an illumination well in addition to that already described.

The autoclave containing the molten hexachlorethane is rotated on the trunnions (5 through the crank 15 until the interface 32 is visible at the center of the sight glass 16,

the water layer 33 being above and the hexa-- chlorethane 34: being below. The valve in the line may then be opened and the water allowed to flow out at an approximate pressure of 150 pounds, preferably into a cold water sump, so that any hexachlorethane escaping with the removal of the water layer As the skimmer extends to the center of the sight glass, it will be l and pressure will vary somewhat within cer-- loo appreciated the water may be selectively drained ofl" to a very fine degree.

After the Water layer has been completely removed, the autoclave may be rotated back to the vertical position and the charge of hexachlorethane allowed to cool and solidify. The mass of hexachlorethane shrinks to a considerable degree in cooling, so that the cover may be removed and the material dumped out when cold by rotating the autoclave.

In Figure 8 there is disclosed a modified form of apparatus for carrying out the in vention. This apparatus comprises a plurality of superimposed containers 35 and 36 having jackets 37 and 38 formed integral therewith as'shown in Figure 3. The lower jacket is provided with an outlet 39 atthe bottom and a similar outlet 41 at the top,

and the jacket 38 likewise provided with a bottom outlet 42 and a top outlet 43.

A member 44 formed of a bowl shaped plate 45 backed against a bowl shaped plate 46 and having a central aperture 47, is interposed between the containers so that it acts as a bottom closure for the upper container 36 and a top closure for the lower container The member 44 is provided in addition with an outer jacket 48 having a plurality of outlets 49 and 51 therein. 7

The lower container 35 is provided with a bottom closure 52 having a conduit 53 formed on one side thereof, adapted to receive an outlet line. The upper container 36 is provided with a dome shaped top closure 54 having a central aperture through-which is inserted-a rod 55. A centrally located tubular extension 56 having an outwardly flanged top .57 is formed on the closure 54. A stufiing gland 58is adapted to be inserted over the rod and seated in the tubular extension 56, which is provided with packing 59. A tapered extension 61 formed in tegral with the stufiing gland having a centrally threaded aperture is mounted on the top of the stuffing gland adapted to be engaged by threads 62 formed on the end of the rod 55.

It will be noted that the rod 55 extends through the central aperture 47 in the member 44. A plug 63 composed of any suitable material not affected by the substances charged into the containers is mounted on the end of the rod and held by a nut 64; A wheel 65 is fixed on the upper end of the rod 55 so that by rotating the same communication between the two containers may be stopped by the plug 63 stopping the aperture 47.

The dome cover 54 is provided in addition with an upwardly extending tubular extension 66 having a flanged top 67, through which material for treatment is charged, and provided with a closure 68 preferably slidably secured thereon by a bolt 69. In the preferred construction, it will be noted that the closure 68- may be held in the opposite side by insertion in a groove provided in the side of the extension 56. It will be apparent, however, that the closure 68 may be fixed over the opening in any other suitable manner so that it may be conveniently removed and replaced.

The jacket 38 on the upper container is connected to the jacket 48 on the member 45 to an elbowed line 71 connected to the outlets 42 and 49 and the jacket 45 connected to the acket 37 on the lower container through a similar line 72 connected to the outlets 51 and 41. A suitable heating medium, such as oil, is preferably charged through the inlet 43 so that it will circulate about the upper container, the member 45 and the lower container, and out of the outlet 39 to heat the contents. of the apparatus.

A pipe 73 having a tapered mouth 74 is positioned in the upper container, having an which is preferably air.

It is apparent that-the apparatus may be provided with the usual temperature and pressure indicating means shown in Figure '1, as well as a pressure control valve of the conventional type. It may also be found desirable to provide a well with a sight glass therein, such as is shown in Figure 1, in the dome cover 54 of the upper container'to allow observation of the liquid levels therein when it is desired to draw oil a certain quantity of liquid through the pipe 73.

This apparatus issuitable for hexachlorethane in the same manner as that already described, shown in Figure 1, although it is of course, as previously explained, susceptible for use with a number of similar materials as well, from which it is desired toremove contained liquids. In treating hexachlorethane, for example, the valve is opened, that is, the plug 63 is positioned as shown in Figure 3, the cover 68 removed, and the hexachlorethane charged through the opening formed by the tubular extension 66.

The material passes on down through the aperture 47 into the lower container. The charging is continued until the lower container is filled, and hexachlorethane added until the upper container is preferably threefourths filled, after which the addition of hexachlorethane is discontinued and the cover replaced and made tight.

Oil or any other suitable heating medium is then introduced, as previously explained,

of the water has been removed, communication between the containers is stopped by manipulation of the hand wheel 65, seating the plug 63 in the aperture 47.

The contents of the chamber 35 may then be allowed to cool to around 185 C. when they may be blown through the conduit 53 by the introduction of air or other pressure medium through the line 77, air preferably being admitted at about 175 pounds per square inch gauge pressure.

A line'79 having a valve 81 interposed therein is connected with the conduit 53 adapted to convey the material from the lower container to a cooling chamber 82 where the hexachlorethane may be subsequently obtained substantially free of moisture. Vhen it is desired to remove the material from thecontainer, such removal may be controlled by the valve 77;

After the charge has been blown from the chamber, the valve 77 is then closed and more heat applied to the charge in the upper chamber,making certain that the hexachlorethane is at least one or two degrees centigrade above its melting points. Communication is then reestablished by'removal of the plug 63 from the aperture 47, further introduction of air through the line 77 being discontinued, permitting the molten hexachlorethane remaining in the upper chamber to pass into the lower chamber together with any small amount of water it may contain, preliminary to repeating the entire process.

There is accomplished by this invention a process and apparatus for removing contained liquids from volatile solvents having a low. intersolubility therewith in the liquid phase withoutany appreciable loss of the normally solid material, and more especially a process and apparatus for drying hexachlorethane without loss of any substantial quantity of the compound.

While I have shown and described the preferred embodiment of my invention, I wish it to be understood that I do not confine myself to the precise deta ls of construction herein set forth, by way of illustration, as it is apparent that many changes and variations may be made therein, by those skilled in the art, without departing from the spirit of the invention, or exceeding the scope of the appended claims.

I claim:

1. An apparatus for removing a contained liquid from a solid, the contained liquid having a low intersolubility with and a diflerent specific gravity than the solid when the latter is in its liquid phase, said apparatus comprising a two compartment container, an upper closure for said container, a discharge line connected to the container, means associated with each compartment for applying heat externally thereto so as to melt the solid, means mounted in one compartment for separately drawing off the liquid of lowest specific gravityafter conversion of the solid into its liquid phase, and means associated with the container for effecting-a closure between the compartments thereof.

2. An apparatus for removing a contained liquid from a solid the contained liquid having a low intersolubility with and a di'fi'erent specific gravity than the solid when the latter is in its liquid phase, said apparatus comprising a vertically mounted container having an upper and lower compartment, an upper closure from the container, a discharge line connected to the lower compartment, said container adapted to be charged with said solid to such an extent that the upper compartment is partially filled therewith, means associated with each compartment for applying heat eX- ternally thereto so as to convert the solid to a liquid, means in the upper compartment for separately drawing ed the liquid of lowest specific gravity after the conversion of the solid to its liquid phase, and means associated with the container for eflecting a closure between the compartments thereof.

3. An apparatus for removing a-contained liquid from a solid, the contained liquid having a low int-ersolubility with and a different specific gravity than the solid when the latter is in its liquid phase, said apparatus comprising a vertically mounted container having an upper and lower compartment therein, an upper closure for the container, a discharge line connected to the lower compartment, said container adapted to be chardged with said solid to such an extent that the upper compartment is partially filled therewith, means associated with each compartment for circulating a heating medium therearound, an angular shaped draw-otf pipe rotatively mounted within the upper compartment, said pipe communicating with the exterior of said c0ntainer, and means associated with the container for effecting a closure between the compartments thereof.

4. An apparatus for removing a contained liquid from a solid, the contained liquid having a low intersolubility with and a different specific gravity than the solid when the latter is in its liquid phase, said apparatus comprising a vertically mounted container having an upper and lower compartment, an upper closure for the container, a discharge line connected to the lower compartment, said container adapted to be charged with said solid to such an extent that the upper compartment is partially filled therewith, means associated with each compartment for applying heat externallv thereto so as to convert the solid to a liquid, means in the upper compartment for separately drawing olf the liquid of lowest specific gravity after the conversion of the solid to the liquid phase, a vertically adjustable rod extending through the upper compartment and into the lower compartment. the lower end of said rod being provided with a closure for shutting ofl" the compartments when the rod is in its elevated position, the upper end of said rod extending through said container, and means mounted upon the container and associated with said rod for raising and lowering it.

5. An apparatus for removing a contained liquid from a solid, the contained liquid having a low intersolubility with and a different specific gravity than the solid when the latter is in its liquid phase, said apparatus comprising a vertically positioned container having its interior restricted at a point near its longitudinal center so as to divide the container into an upper and lower compartment, an upper closure for the container, a draw off line communicating with the lower coinpartment of the container and a closure therefor, a heating jacket surrounding each of said compartments with a pipe connecting the jackets to each other, an angular shaped draw olf pipe rotatively mounted within the upper compartment, said last mentioned pipe communicating with the exterior of said container, a vertically adjustable rod extending a through the upper compartment and into the lower compartment, the lower of said rod being provided with a closure for shutting off the compartments when the rod is in its elevated position, the upper end of said rod extending through said container, and means mounted upon the container and associated with said rod for raising and lowering it.

6. An apparatus for removing a contained liquid from a solid, the contained liquid having a low intersolubility with and a different specific gravity than the solid when the latter is in its liquid phase, said apparatus comprising a two compartment container, an upper closure for said container, a discharge line connected to the container, means associated with each compartment for applying heat externally thereto so as to melt the solid, means mounted in one compartment for separately drawing off the liquid of lowest specific gravity after the conversion of the solid to its liquid phase, means associated with the other compartment for forcing the contents thereof into a discharge line, and means for effecting a closure between the compartments.

7. An apparatus for removing a contained liquid from a solid, the contained liquid having a low intersolubility with and a different specific gravity than the solid when the latter is in its liquid phase, said apparatus comprising a vertically mounted container having an upper and lower compartment, an upper closure for the container, a discharge line connected to the lower compartment, said container adapted to be charged with said solid to such an extent that the upper compartment is partially filled therewith, means associated with each compartment for applying heat externally thereto'so as'to convert the solid to a liquid, means in the upper cor partment for separately drawing olf the liqing a low intersolubility with and a differentspecific gravity than the solid when the latter is in its liquid phase, said apparatus comprising a vertically mounted'container having an upper and lower compartment therein, and upper closure for the container, a discharge line connected to the lower compartment, said container adapted to be charged with saidsolid to such an extentthat the upper compartment is partially filled therewith,

means associated with each compartment for circulating a heating medium therearound,

an angular shaped draw-oil pipe rotatively mounted within the upper compartment, said pipe communicating with the exterior of said container, means associated with the container for effecting a closure between the compartments thereof, and still other'means as sociated with the container for introducing a gas under pressure into the lower compartment to force the contents thereof into said discharge line.

9. An apparatus for removing a contained liquid from a solid, the contained liquid having a low intersolubility with and a different specific gravity than the solid when the latter is in its liquid phase, said apparatus comprising a vertically mounted container having an upper and lower compartment, an upper closure for the container, a discharge line connected to the lower compartment, said container adapted to be charged with said solid to such an extent that the upper compartment is partially filled therewith, means associated with each compartment for applying heat externally thereto so as to convert the solid to a liquid, means in the upper compartment for separately drawing off the liquid of lowest specific gravity after the conversion of the solid to the liquid phase, a vertically adjustable rod extending through the upper compartment and into the lower compartment, the lower end of said rod being provided with a closure for shutting off the compartments when the rod is in its elevated position, the upper end of said rod extending through said container, means mounted upon the container and associated with said rod for raising and.

lowering it, and still other means associated with the container for introducing a gas under pressure into the lower compartment to force the contents thereof into said discharge line.

10. An apparatus for removing a contained liquid from a solid, the contained liquid having a low intersolubility with and a difierent specific gravity than the solid when the latter is in its liquid phase, said apparatus comprising a vertically positioned container havmg its interior restricted at a point near its longitudinal center so as to divide the container into an upper and lower compartment an upper closure for the container, a draw-cit line communicating with the lower compartment of the container and aclosure therefor, a heating jacket surrounding each of said compartments with a pipe connecting the jackets to each other, an angular shaped draw-off pipe rotatively mounted within the upper compartment, said last mentioned pipe communicating with the exterior of said container, a vertically adjustable rod extending through the upper compartment and into the lower compartment, the lower end of said rod being provided with a closure for shutting off 6 the compartments when the rod is in its elevated position, the upper end of said rod extending through said container, means mounted upon the container and associated with said rod for raising and lowering it, and a pipe for introducing a gas under pressure into said container, said pipe being led into said container at a point near the top of said lower compartment.

In testimony whereof I aifix my signature. 6 ROLLAND D. MYERS. 

